HRID509099

反应详情

EQUATION

反应方程式

HRID 509099 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3-Cyano-N-(2,4-dimethoxybenzyl)-4-[2-methoxy-4-(trifluoromethyl)benzyl]-N-1,2,4-thiadiazol-5-ylbenzenesulfonamide (Preparation 30, 33.8 mg, 0.056 mmol) was dissolved in dichloromethane (1 mL) and cooled to 0° C. Trifluoroacetic acid (22 μL, 0.28 mmol) was added and the reaction stirred for 3 hours warming slowly to room temperature. The solvent was removed in vacuo and the residue re-dissolved in methanol (˜5 mL). Once again the solvent was removed in vacuo. The material was suspended in methanol (5 mL) and filtered through Celite™. The reaction mixture was concentrated in vacuo and purified by the B-HPLC method to afford the title compound.

WORKUP

后处理

  1. temperaturewarming slowly to room temperature
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue re-dissolved in methanol (˜5 mL)
  4. customOnce again the solvent was removed in vacuo
  5. filtrationfiltered through Celite™
  6. concentrationThe reaction mixture was concentrated in vacuo
  7. custompurified by the B-HPLC method